Lubricant



Patented Mar. 4, 1941 UNITED STATES PATENT OFFICE No Drawing.Application August 9, 1935. Serial No. 35,516

20 Claims.

This invention relates to lubricants, and has for an object to obtain alubricant having uniform lubricating characteristics such as high loadcarrying capacity, and shock resistance, and. low

power consumption characteristics.

Another object of the invention is to provide possesses hlghloadcarrying capacity and shock resistance, and low power consumptioncharacteristics. This lubricant comprises essentially 20 a minerallubricating oil compounded with a minor proportion of halogenatedhydrocarbons, which may be aliphatic, aromatic, or alicyclic, and aminor proportion of saponifiable, oxygen containing organic compounds.In quantity pro- 5 duction I found, however, that different batches ofmy lubricant, of apparently identical composition, differed inlubricating characteristics.

I have discovered that uniformity, as well as enhanced results can beobtained by heating to 30 high temperatures (for example, 200 C.)preferably with agitation, for a short but sufiicient period of time,such as fifteen minutes, either the components of the improvedlubricant, separately or in groups and mixing preferably while hot or 35above room temperatures, or the compounded lubricant mixture. Fbrexample, an S. A. E. #90

gear lubricant containing 8% of chlorinated naphthalene (carrying about63% chlorine), 2%

of oxidized petroleum acids, and 4% of alpha 4 monochlornaphthaleneapparently will go together completely at 110 C. but the mixture at a'load of 200 pounds gage on a Floyd lubricant tester sometime showsscratching of the test pieces. When heated to 200 C. for fifteen 4minutes, with stirring, the same lubricant carries 200 pounds for fiveminutes, which may be followed by 325 pounds for five minutes, withoutscratching of thetest pieces. The load may then be increased to 600pounds, whereupon the test piece will begin to extrude, the bearingsurfaces being afterward found to be perfectly burnished and free fromscratches. Furthermore, these'results can be duplicated repeatedly.

Certain chlorinated organic compounds (for example aliphatics,alicyclics, etc.) will not withstand these high temperatures withoutdecomposition, and lubricant plants are not ordinarily equipped fordeveloping such high temperatures. After experimentation, therefore, Ihave found that equal results may be obtained at lower temperatures, forexample 100 C., by prolonging the heating time for the lubricant, andits components. In one case, heating sixteen hours at 110 C. gavesatisfactory results. In other cases still lower temperatures aredesirable and practicable. 10 At these relatively low temperatures, avacuum should preferably be used. For example, approximately twenty-nineinches of vacuum applied at approximately 80 C. for a sufiicient timewill develop the desired characteristics.

In all of the above examples, the end result is the same-to developuniform and high qualities, and I have found that the use of heat underproperly controlled conditions develops these desired characteristics.Whether the result secured 2G by this heat treatment is because of theelimination of traces of moisture or some other deleterious constituent,either by volatilization or precipitation, or by the production of aphysical coordination or chemical union between the components of thelubricant, or a combination of these factors,

I am unable at this time to state definitely,but the resultantlubricants have maximum pressure and. minimum friction characteristicsfor the particular combinations used, with little or no change inviscosity.

The heat treatment with agitation appears to homogenize the mixture. Thedegree of heat selected for any particular compound is preferably onewhich is below the temperature at which the g5 ingredients or agents orany of them become unstable. Since the duration of the heating may varyto some extent, depending upon the temperatures used, I prefer tocontinue the heating in each case until samples of the homogenized andtreated mixture taken at successive intervals during the heating orhomogenizing operation, when tested on a lubricant tester, show that themixture has developed the desired and uniform lubricatingcharacteristics, as determined by reference to a. standardspecification. When the components are heated separately the heating iscontinued until samples taken at intervals and homogenized with theother components give similar test indications when the homogenized ytest blends are tested.

While I prefer to mix all the ingredients and homogenize the mixturewith heat until the mixture possesses the desired and uniformlubricating characteristics as above explained, I have found thatbeneficial effects may be obtained by separately heat treating the oiland added agents or ingredients, and then mixing the oil with the agentor agents while hot. The mixture may then be further homogenized, withbeneficial results,

to break down and allow the ingredients to separate.

While the free moisture can be eliminated in any suitable manner, suchas by subjecting the materials to well known chemical moisture removingagents, I have found that the heat treatment is the simplest and mostsatisfactory method of accomplishing the purpose, because the solutionsare formed most readily under the action of heat, and the homogenizingor chemical union of the mixture proceeds more rapidly andsatisfactorily while the mixture is heated. Therefore, I simplify theprocedure by utilizing the heat and agitation, not only to remove thefree moisture but also to accelerate the solution of the ingredients inthe oil and homogenize and/or chemically unite the mixture. If themixture is not heated in order to blend or homogenize the ingredients,or if the free moisture is not eliminated, the added ingredients oragents tend to separate out when the mixture is quiescent in some cases.

In my prior applications hereabove referred to, I have disclosed themixing of a major proportion of a mineral lubricating oil with a minorproportion of a substantial] neutral bodyof oil film strengthening, oilsoluble hydrocarbon having a halogen, such as chlorine, in chemicalcombination therewith, such body being substantially non-volatile atordinary temperatures, and a minor proportion of another body offriction reducing, oil soluble organic compound having oxygen insaponifiable chemical combination therewith. As an example of a neutralbody of hydrocarbon I have mentioned chlorinated naphthalenes,chlorinated diphenyls, chlorinated naphthenes and chlorinated parafiinesto be particularly satisfactory.

Among the friction reducing compounds which may be employed are castoroil, oleic acid, stearic acid, lard oil and Alox. The substancesavailable under the name Alox are manufactured on a commercial scale andare available in the open market under the name Alox. 'I'hey areobtained by the controlled oxidation of parafline hydrocarbons or acidsand contain a variety of compounds which are believed to includelactones, internal anhydrides of hydroxylated compounds, ketones, ketonealcohols, fatty acids, aldehydes, and esters. closed in U. S. Patents toBurwell No. 1,690,769 ranted November 6, 1928, and No. 1,863,004 grantedJune 14, 1932. Reference to those patents may be had for furtheridentification of Such substances are dis- I have found that beneficialeffects can also be obtained by the heat treatment separately of the oiland the Alex or other friction reducing body, or of the chlorinatedhydrocarbon, and then their mixture while hot, or, if desired, any twoof them may be heated and then mixed While hot with the other agent orwith the oil I have also found that the heat treatment improves thesolvent action of the oil for the friction reducing agent and thechlorinated product which may be added, and that this improvementpersists after the oil has returned to ordinary temperatures.

I am .aware that it is old in the art to heat chlorinated aliphatichydrocarbons to a temperature of approximately 300 F. in order to removehydrochloric acid which is unstable at that temperature, but to the bestof my knowledge and belief no one heretofore has ever treated the oiland any or all of the ingredients, either separately or together in themanner hereinabove disclosed in order to improve the lubricatingcharacteristics of the mixture. It is noted, however, that according tothis invention, there is no condensation productor Friedel-Kraftoperation, because there is no production of free hy- 1. In themanufacture of lubricants in which v a halogenated hydrocarbonfilm-strength increasing agent and an oxygen bearing friction reducingagent, are added to increase the effectiveness of the lubricant, themethod of insuring uniform and maximum effectiveness of the lubricantmixture which comprises heating the lubricant and at least one of theagents of the mixture under conditions of temperature and pressure andfor a period of time which will eliminate any free moisture present inthe lubricant and the agents that are heated, and homogenizing themixture while hot.

2. In the manufacture of lubricants, in which a halogenated hydrocarbonfilm-strength increasing agent and an oxygen bearing friction reducingagent, are added to a lubricant in order to increase the effectivenessof the lubricant, the method of insuring uniform and maximumeifectiveness of the lubricant mixture, which com prises removing freemoisture from the lubricant and each of said added agents, andhomogenizing the mixture while hot. i

3. In the manufacture of lubricants, in which a halogenatedhydrocarbonfilm-strength increasing agent and an oxygen bearing frictionreducincrease the effectiveness of the lubricant, the method ofinsuring. uniform and maximum effectiveness of the lubricant r ix-ture,which comprises heating the lubricant and at least one of the agents ofthe mixture inder conditions of temperature which will eliminate anyfree moisture present, and which temperature is below that at which thelubricant and any agent of the mixture become unstable, and homogenizingthe mixture while hot.

4. In the manufacture of lubricants in which a halogenated hydrocarbonfilm-strength increasing agent and an oxygen bear ing friction acompound of high film strength and lower coconditions of temperature andpressure and for a period of time'which will eliminate any free moisturepresent in the lubricant and the agents that are heated, andhomogenizing the mixture I while hot.

5. In the manufacture of lubricants, in which a halogenated hydrocarbonfilm-strength increasing agent and an oxygen bearing friction reducingagent are added to a lubricant in order to increase the effectiveness ofthe lubricant, the method of insuring uniform and maximum effectivenessof the lubricant mixture, which comprises mixing the lubricant with oneof said agents under anhydrous conditions, and homogenizing the mixturewhile hot until the agent is thoroughly blended throughout the lubricantand does not materially separate therefrom upon standing, and adding theother agent.

6. In the manufacture of lubricants, in which a halogenated hydrocarbonfilm-strength increasing agent and an oxygen bearing friction reducingagent are added to a lubricant in order to increase the effectiveness ofthe lubricant, the method of insuring uniform and maximum effectivenessof the lubricant mixture, which comprises subjecting the lubricant andthe added agents to heat under such pressure conditions and for suchperiod of time as will eliminate any free moisture present in thelubricant and the agents, but with the temperature below that at whichthe mixture and the components thereof become unstable, and homogenizingthe mixture while hot.

7. In the manufacture of lubricants to obtain a compound of high filmstrength and lower coefiicient of friction over a significant range ofworking conditions than any one of its constituents or any two of itsconstituents combined, the method which comprises heating a majorproportion of a lubricating oil, a minor proportion of a substantiallyneutral body of oil film strengthening, oil soluble hydrocarbon havinghalogen in chemical combination therewith, and a minor proportion ofanother body of friction reducing oil soluble organic compound havingoxygen in saponifiable chemical combination therewith,'under conditionsof temperature and pressure and for a period of time which wouldeliminate free moisture in any of the constituents, and homogenizing themixture.

8. In the manufacture of lubricants to obtain a compound of high filmstrength and lower coefficient of friction over a significant range ofworking conditions than any one of its constituents or any two of itsconstituents combined, the method which comprises heating together amajor proportion of a mineral lubricating oil, a minor proportion of afriction reducing, oil soluble organic compound having oxygen insaponifiable chemical combination therewith, and a minor proportion ofanother and substantially neutral body of oil film strengthening, oil

soluble hydrocarbon having halogen in chemical combination therewith,until tests on a lubricant tester of samples thereof taken at successiveintervals during the heating show maximum and substantially uniform filmstrength and minimumand uniform friction characteristics.

9. In the manufacture of lubricants to obtain eflicient of friction overa significant range of working conditions than any one of itsconstituents or any two of its constituents combined, the method whichcomprises heating a major proportion of a mineral lubricating oil, and aminor proportion of a friction reducing oil soluble organic compoundhaving oxygen in saponifiable chemical combination therewith, andhomogenfing the mixture with a halogenated hydrocar- 10. In themanufacture of lubricants to obtain a compound of high film strength andlower coefficient of friction over a significant range of workingconditions than any one of its constituents or any two of itsconstituents combined, the

- nfethod which comprises heating a major proportion of a lubricatingoil, a minor proportion of a friction reducing oil soluble organiccompound having oxygen in saponifiable chemical combination therewith,and a minor proportion of another and substantially neutral body of oilfilm strengthening, oil soluble hydrocarbon having halogen in chemicalcombination therewith, and homogenizing the mixture with heat untiltests on a lubricant tester of samples thereof taken at successiveintervals during the heating show maximum and substantially uniform filmstrength and minimum and uniform friction characteristics.

11. A lubricant compound of high film strength and lower coefficient offriction over a significant range of working conditions than any one ofits constituents or an two of its constituents combined, comprising amajor proportion of lubricating oil having dissolved therein a minorproportion ,of a substantially neutral body of oil film strengthening,oil soluble. hydrocarbon having a halogen in chemical combinationtherewith, and a minor proportion of another body of friction reducing,oil soluble organic compound having oxygen in saponifiable chemicalcombination therewith, said oil, said hydrocarbon and said frictionreducing compound being homogenized under anhydrous conditions untilsamples thereof taken at successive intervals during the homogenizingoperation and tested on a lubricant tester show maximum andsubstantially uniform film strength and minimum and uniform friction.

12. A lubricant compound of high film strength and lower coefficient offriction over a significant range of working conditions than any one ofits constituents or any two of its constituents combined, comprising amajor proportion of lubricating oil having dissolved therein a minorproportion of a substantially neutral body of oil film strengthening,oil soluble'hydrocarbon having a halogenin chemical combinationtherewith, and a minor proportion of another body of friction reducing,oil soluble organic compound having oxygen in saponifiable chemicalcombination therewith, said oil, said hydrocarbon and said frictionreducing compound being homogenized while heated under anhydrousconditions until samples thereof taken at successive intervals duringthe heating and tested on a lubricant tester show maximum andsubstantially unchanging film strength and minimum and unchangingfriction.

13. In the manufacture of extreme pressure lubricants in which ahalogenated, hydrocarbon, film-strength increasing agent and an oxygenbearing, friction reducing agent are added to a lubricant to increasepermanently the lubricating effectiveness thereof, and the halogen andoxygen of said agents are in separate molecules, the method of insuringuniform and maximum effectiveness of the lubricant mixture whichcomprises heating the basic lubricant and at least one of the addedagentsunder selected conditions of temperature and pressure until testson a lubricant tester of samples of the complete mixture of thelubricant and added agents prepared from portions taken at successiveintervals from the heated mixture during the heating show maximum andsubstantially uniform film strength and minimum and uniform frictioncharacteristics.

14. In the manufacture of extreme pressure lubricants in which ahalogenated, hydrocarbon, film-strength increasing agent and an oxygenbearing, friction reducing agent are added to a lubricant to increasepermanently the lubricating, efiectiveness thereof, and the halogen andoxygen of said agents are in separate molecules, the method of insuringuniform and maximum effectiveness of the lubricant mixture whichcomprises heating at least one of the ingredients of the'mixture untiltests on a lubricant tester of samples of the homogenized mixture of allingredients including the heated ingredient show substantially no changein the film strength and friction characteristics upon further heatingof said heated ingredient.

15. In the manufacture of extreme pressure lubricants in which ahalogenated, hydrocarbon, film-strength increasing agent and an oxygenbearing, friction reducing agent are added to a lubricant to increasepermanently the lubricating effectiveness thereof, and the halogen andoxygenof said agents are in separate molecules, the method insuringuniform and maximum effectiveness of the lubricant mixture whichcomprises heating and agitating at least two of the ingredients of themixture until tests on a lubricant tester of samples of the homogenizedmixture of all ingredients including the heated and agitated ingredientsshow substantially no further improvement in the lubricatingcharacteristics of the samples upon further heating of said heatedingredients.

16. A lubricant compound of permanent high film strength and lowercoefiicient of friction over a significant range of working conditionsthan any one of its constituents or ,any two of its constituentscombined, comprising a major proportion of lubricating oil havingdissolved therein a minor proportion of a halogenated, hydrocarbon filmstrength increasing agent and an oxygen bearing friction reducing agent,with the halogen and oxygen in separate? molecules, said solution beinghomogenized while heated until samples thereof taken at successiveintervals during the heating and tested on a lubricant tester showsubstantially no change in lubricating properties.

17. A lubricant compound of permanent high fihn strength and lowercoeflicient of friction aaaes I over a significant range of workingconditions than any one of -its constituents or any two 01' itsconstituents combined, comprising a major proportion of lubricating oilhaving dissolved- 18. A lubricant compound of permanent high filmstrength and lower coefficierit of friction over a significant range ofworking conditions than any one of its constituents or any two of itsconstituents combined, comprising a major proportion of lubricating oilhaving dissolved therein a, minor proportion of a halogenated,hydrocarbon film strength increasing agent and an oxygen bearingfriction reducing agent, with the halogen and oxygen in separatemolecules, at least two of the constituents of said compound beingheated, at a temperature at which they remain chemically stable, forsuch interval that a homogenized mixture of the constituents of thecompound including the heated constituents,

when tested on a lubricant tester shows unchanging lubricatingproperties when the mixture is further heated.

19. In the manufacture of extreme pressure lubricants in which ahalogenated, hydrocarbon, film-strength increasing agent and an oxygenbearing, friction reducing agent are added'to a lubricant to increasepermanently the lubricating effectiveness thereof, and the halogen andoxygen of said agents are in separate molecules, the method of insuringuniform and maximum effectiveness of the lubricant mixture whichcomprises heating the basic lubricant and at least one of the addedagents for a minimum period of time depending upon the temperature andvaryin from a period of approximately 15 minutes at approximately 200 C.to approximately sixteen hours at approximately- C.

20.111 the manufacture of extreme pressure lubricants in which ahalogenated, hydrocarbon,

film-strength increasing agent and an oxygen bearing, friction reducingagent are added to d 'minimum period of time depending upon thetemperature and varying from a period of approximately 15 minutes atapproximately 200 C. to approximately sixteen hours at approximately 110C. i

WILLIAM ALVAH SMI'I'H.

